CN110041541B - Method for processing polymer conductive film - Google Patents
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- 229920000642 polymer Polymers 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims description 11
- 238000012545 processing Methods 0.000 title claims description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000013078 crystal Substances 0.000 claims abstract description 28
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 22
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 19
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 15
- BKNNXPZCASTCIE-UHFFFAOYSA-N 6-(4-methoxyphenoxy)hexanoic acid Chemical compound COC1=CC=C(OCCCCCC(O)=O)C=C1 BKNNXPZCASTCIE-UHFFFAOYSA-N 0.000 claims abstract description 13
- ZDSLGOYLPJYLKU-UHFFFAOYSA-N COc1cc(CBr)c(OCCCCCC(O)=O)cc1CBr Chemical compound COc1cc(CBr)c(OCCCCCC(O)=O)cc1CBr ZDSLGOYLPJYLKU-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000725 suspension Substances 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 238000003672 processing method Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 62
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 40
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 37
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 36
- 239000007787 solid Substances 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 35
- 239000012153 distilled water Substances 0.000 claims description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 24
- 229910052725 zinc Inorganic materials 0.000 claims description 23
- 239000011701 zinc Substances 0.000 claims description 23
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 20
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 20
- 238000002844 melting Methods 0.000 claims description 20
- 230000008018 melting Effects 0.000 claims description 20
- 238000001291 vacuum drying Methods 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 16
- 238000007254 oxidation reaction Methods 0.000 claims description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 239000002270 dispersing agent Substances 0.000 claims description 14
- 239000012065 filter cake Substances 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 12
- 238000010992 reflux Methods 0.000 claims description 12
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 229960000583 acetic acid Drugs 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 238000003760 magnetic stirring Methods 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 8
- 238000000967 suction filtration Methods 0.000 claims description 8
- 239000003513 alkali Substances 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 5
- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 0.000 claims description 4
- NVRVNSHHLPQGCU-UHFFFAOYSA-N 6-bromohexanoic acid Chemical compound OC(=O)CCCCCBr NVRVNSHHLPQGCU-UHFFFAOYSA-N 0.000 claims description 4
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 4
- 239000012295 chemical reaction liquid Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 239000012362 glacial acetic acid Substances 0.000 claims description 4
- LHGVFZTZFXWLCP-UHFFFAOYSA-N guaiacol Chemical compound COC1=CC=CC=C1O LHGVFZTZFXWLCP-UHFFFAOYSA-N 0.000 claims description 4
- 239000005457 ice water Substances 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000006386 neutralization reaction Methods 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 4
- 230000010355 oscillation Effects 0.000 claims description 4
- 230000020477 pH reduction Effects 0.000 claims description 4
- 229920002866 paraformaldehyde Polymers 0.000 claims description 4
- 235000011837 pasties Nutrition 0.000 claims description 4
- LPNYRYFBWFDTMA-UHFFFAOYSA-N potassium tert-butoxide Chemical compound [K+].CC(C)(C)[O-] LPNYRYFBWFDTMA-UHFFFAOYSA-N 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 239000008117 stearic acid Substances 0.000 claims description 4
- 239000010959 steel Substances 0.000 claims description 4
- 238000006277 sulfonation reaction Methods 0.000 claims description 4
- 238000004381 surface treatment Methods 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000012495 reaction gas Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims 3
- 238000012423 maintenance Methods 0.000 claims 1
- 235000011187 glycerol Nutrition 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 8
- 229910052751 metal Inorganic materials 0.000 abstract description 7
- 239000002184 metal Substances 0.000 abstract description 7
- 239000000945 filler Substances 0.000 abstract description 6
- 239000000843 powder Substances 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 35
- 239000000463 material Substances 0.000 description 13
- 230000001276 controlling effect Effects 0.000 description 9
- PEEHTFAAVSWFBL-UHFFFAOYSA-N Maleimide Chemical compound O=C1NC(=O)C=C1 PEEHTFAAVSWFBL-UHFFFAOYSA-N 0.000 description 6
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 6
- JFATZQWHTPPTEJ-UHFFFAOYSA-N 6-methylheptan-3-yl 2-sulfanylpropanoate Chemical compound SC(C(=O)OC(CC)CCC(C)C)C JFATZQWHTPPTEJ-UHFFFAOYSA-N 0.000 description 5
- 229920001940 conductive polymer Polymers 0.000 description 4
- 229920000547 conjugated polymer Polymers 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 239000011231 conductive filler Substances 0.000 description 2
- 230000021615 conjugation Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- ZHUWXKIPGGZNJW-UHFFFAOYSA-N 6-methylheptyl 3-sulfanylpropanoate Chemical compound CC(C)CCCCCOC(=O)CCS ZHUWXKIPGGZNJW-UHFFFAOYSA-N 0.000 description 1
- 239000004734 Polyphenylene sulfide Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
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- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- -1 polyphenylene acetylene Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 229920000123 polythiophene Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- C08G61/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G61/12—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule
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- C08G2261/30—Monomer units or repeat units incorporating structural elements in the main chain
- C08G2261/34—Monomer units or repeat units incorporating structural elements in the main chain incorporating partially-aromatic structural elements in the main chain
- C08G2261/344—Monomer units or repeat units incorporating structural elements in the main chain incorporating partially-aromatic structural elements in the main chain containing heteroatoms
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- C08K5/00—Use of organic ingredients
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Abstract
The invention discloses a processing method of a polymer conductive film, which solves the problems that the existing polymer conductive film is difficult to form a film, and the conductivity is influenced because a metal powder filler is easy to oxidize after being used for a long time, and comprises the following steps: synthesis of 1-methoxy-4 (5 '-carboxypentyloxy) benzene, synthesis of 1, 4-dibromomethyl-2-methoxy-5 (5' -carboxypentyloxy) benzene, synthesis of MDP-PPV, preparation of MDP-PPV methanol solution and preparation of ZnOwForming the whisker suspension and the polymer conductive film. The invention takes MDP-PPV as a film forming matrix and ZnO aswThe crystal whisker is used as a filler, and a certain amount of glycerin and a release agent are added, so that the convenience of film formation is rapidly improved, and the conductivity of the polymer conductive film is also effectively improved.
Description
Technical Field
The invention relates to the technical field of conductive film processing, in particular to a method for processing a polymer conductive film.
Background
A large number of conjugated polymers, such as polyaniline, polypyrrole, polythiophene, polyphenylene acetylene, polyphenylene sulfide, etc., have been discovered in succession, and after doping, the conductivity can reach the level of semiconductors or even metal conductors. The appearance of the conductive polymer not only lays a foundation for the generation of low-dimensional electronics, but also has a special structure and excellent physical and chemical properties, so that the conductive polymer has wide and attractive application prospects in the fields of energy sources, optoelectronic devices, information storage, transmission and processing, sensors, electromagnetic shielding, metal corrosion prevention and stealth technologies. Especially in the aspect of stealth technology, the conductive polymer has low density, can be made into a very thin film, generates very small additional weight, and can overcome the defect of large additional weight of inorganic stealth materials. Therefore, conductive polymers have been the focus of research in material science since the discovery. However, the conventional polymer conductive film is difficult to form, and the metal powder filler is easily oxidized after a long time use, which affects the conductivity, so that it is necessary to design a processing method of the polymer conductive film.
Disclosure of Invention
Aiming at the situation, in order to overcome the defects of the prior art, the invention provides the processing method of the polymer conductive film, which effectively solves the problems that the existing polymer conductive film is difficult to form a film, and the metal powder filler is easy to oxidize and influences the conductivity after being used for a long time.
In order to achieve the above object, the present invention comprises the steps of:
s1, Synthesis of 1-methoxy-4 (5' -carboxypentyloxy) benzene: dissolving 400 plus 600ml of sodium hydroxide in ethanol by magnetic stirring and ultrasonic oscillation, slowly dropwise adding the solution into 6-bromohexanoic acid/ethanol solution which is placed in ice water bath and continuously stirred, obtaining white pasty solid after dropwise adding, adding a proper amount of distilled water for dissolving for later use after stirring for 40-45min, firstly introducing ammonia gas for 30min in a three-neck flask which is provided with a stirrer and a reflux condenser tube, adding 100 plus 150ml of sodium hydroxide and distilled water under the protection of the ammonia gas, adding 80-85ml of methoxyphenol and the prepared solution for later use after stirring and dissolving at room temperature, reacting for 22h in an oil bath at 60 ℃, dropwise adding hydrochloric acid for acidification after the reaction is finished, adjusting the pH of the reaction solution to be 1-2, cooling the reaction solution to room temperature, precipitating white solid in the flask, performing suction filtration, repeatedly washing a filter cake to be neutral by the distilled water, vacuum drying at 50 deg.C to obtain white needle sheet crystal, and recrystallizing the obtained solid with anhydrous ethanol to obtain 1-methoxy-4 (5' -carboxypentyloxy) benzene;
synthesis of S2, 1, 4-dibromomethyl-2-methoxy-5 (5' -carboxypentyloxy) benzene: introducing ammonia gas for 0.5h into a three-neck flask provided with a stirrer and a condenser, adding 200-220ml of 1-methoxy-4 (5 '-carboxyl pentoxy) benzene and glacial acetic acid solution, refluxing and stirring for 0.5h under the protection of ammonia gas, after the solution is dissolved, rapidly adding 100-120ml of paraformaldehyde and hydrobromic acid/acetic acid solution, refluxing and reacting for 12h in an oil bath at 85 ℃, pouring the reaction solution into 1000ml of distilled water after the reaction is finished, separating out a large amount of solid, performing suction filtration, repeatedly washing with distilled water until the filter cake is neutral, placing the filter cake at 55 ℃ for vacuum drying to obtain a light yellow granular solid, introducing anhydrous ethanol to dissolve the obtained solid, sequentially washing with a 5% sodium carbonate solution and saturated saline water, and drying with anhydrous sodium sulfate to remove the solvent to obtain the light yellow solid, namely the 1, 4-dibromomethyl-2-methoxy-5 (5' -carboxyl pentoxy) benzene;
s3, synthesis of MDP-PPV: introducing ammonia gas into a three-neck flask provided with a stirrer and a condenser for 0.5h, adding 50-60ml of potassium tert-butoxide and refined anhydrous tetrahydrofuran, stirring and dissolving in an oil bath at 70 ℃, then slowly dropwise adding an anhydrous tetrahydrofuran solution of 1, 4-dibromomethyl-2-methoxy-5 (5' -carboxypentyloxy) benzene, gradually changing the solution into red, slowly deepening the color, after the dropwise adding, continuously heating and stirring for 3-4h, after the reaction is finished, dropwise adding 10ml of distilled water into the reaction liquid, centrifugally separating to obtain a red solid, extracting the red solid with tetrahydrofuran for one week, and vacuum drying at 50 ℃ to obtain a polymer MDP-PPV;
s4, preparing an MDP-PPV methanol solution: putting the polymer MDP-PPV into a vacuum drying oven for drying for 24h, putting the dried polymer MDP-PPV into absolute ethyl alcohol, magnetically stirring for 24h, filtering by a microporous filter to remove insoluble substances, and preparing an MDP-PPV methanol solution;
s5, preparing ZnOwWhisker suspension: 5ml of surface-treated ZnOwAdding crystal whisker into 30ml boiling water, adding 0.25ml dispersant, and keeping for 45-55min under magnetic stirring to make ZnOwThe crystal whisker is fully dispersed to prepare ZnOwA suspension of whiskers, wherein said ZnOwThe preparation method of the crystal whisker comprises the steps of firstly adding zinc powder into distilled water, adding a proper amount of hydrogen peroxide, stirring for 2-3h by a motor, then standing for 72h at room temperature, filtering, drying for 4-6h at 100 ℃ to obtain pretreated zinc powder, continuously adding the pretreated zinc powder into a melting tank of a melting furnace, melting the zinc liquid in the melting tank, controlling the temperature in the melting furnace to be 420-750 ℃, then introducing the molten zinc liquid into an evaporation tank of a steam generation furnace through a zinc liquid conduit, and controlling the temperature in the steam generation furnace to be 1050 DEG CObtaining zinc vapor, then leading the zinc vapor into an oxidation reaction furnace through a zinc vapor guide pipe after the zinc vapor overflows an evaporation tank, controlling the temperature in the oxidation reaction furnace to be 900-1500 ℃, enabling the zinc vapor to be in contact with oxygen-containing gas in the oxidation reaction furnace to carry out oxidation reaction, controlling the reaction gas conditions in the oxidation reaction furnace to generate micron or nano ZnOwWhisker;
s6, forming of the polymer conductive film: in a three-neck flask equipped with a stirrer and a condenser, the MDP-PPV methanol solution and ZnO are addedwAdding the whisker suspension, glycerol and a parting medium into a flask according to the proportion of 7:3:1:1, heating in water bath at 70-80 ℃ for 25-30min at the rotating speed of 2000-2200r/min, standing at room temperature for 3-5min, filtering, coating on a steel plate, drying in an electrothermal constant-temperature drying oven at 80-90 ℃ for 20-25min, taking out, standing at room temperature for 10min, and removing the membrane to obtain the polymer conductive membrane.
According to the technical scheme, the dispersing agent is prepared from the following raw materials in parts by weight: 20-35 parts of washing oil, 10-15 parts of sulfuric acid, 15-20 parts of formaldehyde, 9-13 parts of liquid alkali, 2-5 parts of maleimide, 3-5 parts of isooctyl 3-mercaptopropionate and 0.2-0.4 part of regulating assistant.
According to the technical scheme, the preparation method of the dispersing agent comprises the steps of firstly adding given amount of washing oil into a sulfonation condensation kettle, starting stirring, heating to 60-70 ℃, dropwise adding given amount of sulfuric acid for 1 hour, slowly heating to 115-120 ℃, vacuumizing, keeping the negative pressure at 0.05MPa, keeping the temperature for 2 hours, then cooling to 70 ℃, dropwise adding given amount of formaldehyde, maleimide, 3-isooctyl mercaptopropionate and an adjusting aid for 0.5 hour, slowly heating to 80-90 ℃, keeping the temperature for 3-4 hours, keeping the temperature, introducing into a neutralization pot, adding liquid alkali to adjust the pH to 6-7, introducing into a filter press after adjustment, and drying filtrate in a vacuum drying box at 70-80 ℃ for 2-3 hours to obtain the dispersing agent.
According to the technical scheme, the ZnOwThe surface treatment method of the crystal whisker comprises the step of treating ZnOwAdding the crystal whisker into a mixed solution prepared by KH-570 and stearic acid according to the proportion of 2:3, stirring at normal temperature at 800-.
The invention takes MDP-PPV asFilm-forming substrate with ZnOwThe crystal whisker is used as a filler, a certain amount of glycerin and a release agent are added at the same time, the MDP-PPV material is a typical conjugated polymer material, and the MDP-PPV material has good film forming property and processability due to high conjugation of a molecular main chain, and ZnO is adoptedwAs the material for preparing the polymer conductive film, because the material has a four-needle-shaped three-dimensional space structure, 4 extended needle-shaped crystal parts of the material can be effectively contacted with the needle-shaped parts of adjacent whiskers to form a good three-dimensional conductive network, so that the material has better conductive performance, and ZnOwCompared with metal powder conductive filler, the conductive film has the advantages that the problem of conductivity reduction caused by the formation of an oxide film on the surface of metal particles after long-term use does not exist, the adaptability of the conductive film to the environment is improved, glycerin and a release agent are added during film forming, the formed film is conveniently and quickly removed, and the use convenience is effectively improved.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a flow chart of a method for processing a polymer conductive film according to the present invention.
Detailed Description
The following describes the present invention in further detail with reference to fig. 1.
Example 1: referring to fig. 1, the present invention provides a technical solution: the processing method of the polymer conductive film comprises the following steps:
s1, Synthesis of 1-methoxy-4 (5' -carboxypentyloxy) benzene: dissolving 400 plus 600ml of sodium hydroxide in ethanol by magnetic stirring and ultrasonic oscillation, slowly dropwise adding the solution into 6-bromohexanoic acid/ethanol solution which is placed in ice water bath and continuously stirred, obtaining white pasty solid after dropwise adding, adding a proper amount of distilled water for dissolving for later use after stirring for 40-45min, firstly introducing ammonia gas for 30min in a three-neck flask which is provided with a stirrer and a reflux condenser tube, adding 100 plus 150ml of sodium hydroxide and distilled water under the protection of the ammonia gas, adding 80-85ml of methoxyphenol and the prepared solution for later use after stirring and dissolving at room temperature, reacting for 22h in an oil bath at 60 ℃, dropwise adding hydrochloric acid for acidification after the reaction is finished, adjusting the pH of the reaction solution to be 1-2, cooling the reaction solution to room temperature, precipitating white solid in the flask, performing suction filtration, repeatedly washing a filter cake to be neutral by the distilled water, vacuum drying at 50 deg.C to obtain white needle sheet crystal, and recrystallizing the obtained solid with anhydrous ethanol to obtain 1-methoxy-4 (5' -carboxypentyloxy) benzene;
synthesis of S2, 1, 4-dibromomethyl-2-methoxy-5 (5' -carboxypentyloxy) benzene: introducing ammonia gas for 0.5h into a three-neck flask provided with a stirrer and a condenser, adding 200-220ml of 1-methoxy-4 (5 '-carboxyl pentoxy) benzene and glacial acetic acid solution, refluxing and stirring for 0.5h under the protection of ammonia gas, after the solution is dissolved, rapidly adding 100-120ml of paraformaldehyde and hydrobromic acid/acetic acid solution, refluxing and reacting for 12h in an oil bath at 85 ℃, pouring the reaction solution into 1000ml of distilled water after the reaction is finished, separating out a large amount of solid, performing suction filtration, repeatedly washing with distilled water until the filter cake is neutral, placing the filter cake at 55 ℃ for vacuum drying to obtain a light yellow granular solid, introducing anhydrous ethanol to dissolve the obtained solid, sequentially washing with a 5% sodium carbonate solution and saturated saline water, and drying with anhydrous sodium sulfate to remove the solvent to obtain the light yellow solid, namely the 1, 4-dibromomethyl-2-methoxy-5 (5' -carboxyl pentoxy) benzene;
s3, synthesis of MDP-PPV: introducing ammonia gas into a three-neck flask provided with a stirrer and a condenser for 0.5h, adding 50-60ml of potassium tert-butoxide and refined anhydrous tetrahydrofuran, stirring and dissolving in an oil bath at 70 ℃, then slowly dropwise adding an anhydrous tetrahydrofuran solution of 1, 4-dibromomethyl-2-methoxy-5 (5' -carboxypentyloxy) benzene, gradually changing the solution into red, slowly deepening the color, after the dropwise adding, continuously heating and stirring for 3-4h, after the reaction is finished, dropwise adding 10ml of distilled water into the reaction liquid, centrifugally separating to obtain a red solid, extracting the red solid with tetrahydrofuran for one week, and vacuum drying at 50 ℃ to obtain a polymer MDP-PPV;
s4, preparing an MDP-PPV methanol solution: putting the polymer MDP-PPV into a vacuum drying oven for drying for 24h, putting the dried polymer MDP-PPV into absolute ethyl alcohol, magnetically stirring for 24h, filtering by a microporous filter to remove insoluble substances, and preparing an MDP-PPV methanol solution;
s5, preparing ZnOwWhisker suspension: 5ml of surface-treated ZnOwAdding crystal whisker into 30ml boiling water, adding 0.25ml dispersant, and keeping for 45-55min under magnetic stirring to make ZnOwThe crystal whisker is fully dispersed to prepare ZnOwSuspension of whiskers in which ZnOwThe preparation method of the crystal whisker comprises the steps of firstly adding zinc powder into distilled water, adding a proper amount of hydrogen peroxide, stirring for 2-3h by a motor, then standing for 72h at room temperature, filtering, drying for 4-6h at 100 ℃ to obtain pre-treated zinc powder, continuously adding the pre-treated zinc powder into a melting tank of a melting furnace, melting into zinc liquid in the melting tank, controlling the temperature in the melting furnace to be 420-750 ℃, then introducing the molten zinc liquid into an evaporation tank of a steam generation furnace through a zinc liquid conduit, controlling the temperature in the steam generation furnace to be 1050 ℃ to obtain zinc steam, then introducing the zinc steam into an oxidation reaction furnace through a zinc steam conduit after overflowing the evaporation tank, controlling the temperature in the oxidation reaction furnace to be 900-1500 ℃, contacting the zinc steam with oxygen-containing gas in the oxidation reaction furnace to perform oxidation reaction, and controlling the reaction gas conditions in the oxidation reaction furnace, formation of micro-or nano-sized ZnOwWhisker;
s6, forming of the polymer conductive film: in a three-neck flask equipped with a stirrer and a condenser, the MDP-PPV methanol solution and ZnO are addedwAdding the whisker suspension, glycerol and a parting medium into a flask according to the proportion of 7:3:1:1, heating in water bath at 70-80 ℃ for 25-30min at the rotating speed of 2000-2200r/min, standing at room temperature for 3-5min, filtering, coating on a steel plate, drying in an electrothermal constant-temperature drying oven at 80-90 ℃ for 20-25min, taking out, standing at room temperature for 10min, and removing the membrane to obtain the polymer conductive membrane.
According to the technical scheme, the dispersing agent is prepared from the following raw materials in parts by weight: 20 parts of washing oil, 10 parts of sulfuric acid, 15 parts of formaldehyde, 9 parts of liquid alkali, 2 parts of maleimide, 3 parts of 3-isooctyl mercaptopropionate and 0.2 part of regulating assistant.
According to the technical scheme, the preparation method of the dispersing agent comprises the steps of firstly adding given amount of washing oil into a sulfonation condensation kettle, starting stirring, heating to 60-70 ℃, dropwise adding given amount of sulfuric acid for 1 hour, slowly heating to 115-120 ℃, vacuumizing, keeping the negative pressure at 0.05MPa, keeping the temperature for 2 hours, then cooling to 70 ℃, dropwise adding given amount of formaldehyde, maleimide, 3-isooctyl mercaptopropionate and an adjusting aid for 0.5 hour, sealing equipment after the addition, slowly heating to 80-90 ℃, keeping the temperature for 3-4 hours, keeping the temperature, introducing into a neutralization pot, adding liquid alkali to adjust the pH to 6-7, introducing into a filter press after the adjustment, and drying filtrate in a vacuum drying box at 70-80 ℃ for 2-3 hours to obtain the dispersing agent.
According to the technical scheme, ZnOwThe surface treatment method of the crystal whisker comprises the step of treating ZnOwAdding the crystal whisker into a mixed solution prepared by KH-570 and stearic acid according to the proportion of 2:3, stirring at normal temperature at 800-.
Example 2: referring to fig. 1, the present invention provides a technical solution: the processing method of the polymer conductive film comprises the following steps:
s1, Synthesis of 1-methoxy-4 (5' -carboxypentyloxy) benzene: dissolving 400 plus 600ml of sodium hydroxide in ethanol by magnetic stirring and ultrasonic oscillation, slowly dropwise adding the solution into 6-bromohexanoic acid/ethanol solution which is placed in ice water bath and continuously stirred, obtaining white pasty solid after dropwise adding, adding a proper amount of distilled water for dissolving for later use after stirring for 40-45min, firstly introducing ammonia gas for 30min in a three-neck flask which is provided with a stirrer and a reflux condenser tube, adding 100 plus 150ml of sodium hydroxide and distilled water under the protection of the ammonia gas, adding 80-85ml of methoxyphenol and the prepared solution for later use after stirring and dissolving at room temperature, reacting for 22h in an oil bath at 60 ℃, dropwise adding hydrochloric acid for acidification after the reaction is finished, adjusting the pH of the reaction solution to be 1-2, cooling the reaction solution to room temperature, precipitating white solid in the flask, performing suction filtration, repeatedly washing a filter cake to be neutral by the distilled water, vacuum drying at 50 deg.C to obtain white needle sheet crystal, and recrystallizing the obtained solid with anhydrous ethanol to obtain 1-methoxy-4 (5' -carboxypentyloxy) benzene;
synthesis of S2, 1, 4-dibromomethyl-2-methoxy-5 (5' -carboxypentyloxy) benzene: introducing ammonia gas for 0.5h into a three-neck flask provided with a stirrer and a condenser, adding 200-220ml of 1-methoxy-4 (5 '-carboxyl pentoxy) benzene and glacial acetic acid solution, refluxing and stirring for 0.5h under the protection of ammonia gas, after the solution is dissolved, rapidly adding 100-120ml of paraformaldehyde and hydrobromic acid/acetic acid solution, refluxing and reacting for 12h in an oil bath at 85 ℃, pouring the reaction solution into 1000ml of distilled water after the reaction is finished, separating out a large amount of solid, performing suction filtration, repeatedly washing with distilled water until the filter cake is neutral, placing the filter cake at 55 ℃ for vacuum drying to obtain a light yellow granular solid, introducing anhydrous ethanol to dissolve the obtained solid, sequentially washing with a 5% sodium carbonate solution and saturated saline water, and drying with anhydrous sodium sulfate to remove the solvent to obtain the light yellow solid, namely the 1, 4-dibromomethyl-2-methoxy-5 (5' -carboxyl pentoxy) benzene;
s3, synthesis of MDP-PPV: introducing ammonia gas into a three-neck flask provided with a stirrer and a condenser for 0.5h, adding 50-60ml of potassium tert-butoxide and refined anhydrous tetrahydrofuran, stirring and dissolving in an oil bath at 70 ℃, then slowly dropwise adding an anhydrous tetrahydrofuran solution of 1, 4-dibromomethyl-2-methoxy-5 (5' -carboxypentyloxy) benzene, gradually changing the solution into red, slowly deepening the color, after the dropwise adding, continuously heating and stirring for 3-4h, after the reaction is finished, dropwise adding 10ml of distilled water into the reaction liquid, centrifugally separating to obtain a red solid, extracting the red solid with tetrahydrofuran for one week, and vacuum drying at 50 ℃ to obtain a polymer MDP-PPV;
s4, preparing an MDP-PPV methanol solution: putting the polymer MDP-PPV into a vacuum drying oven for drying for 24h, putting the dried polymer MDP-PPV into absolute ethyl alcohol, magnetically stirring for 24h, filtering by a microporous filter to remove insoluble substances, and preparing an MDP-PPV methanol solution;
s5, preparing ZnOwWhisker suspension: 5ml of surface-treated ZnOwAdding crystal whisker into 30ml boiling water, adding 0.25ml dispersant, and keeping for 45-55min under magnetic stirring to make ZnOwThe crystal whisker is fully dispersed to prepare ZnOwSuspension of whiskers in which ZnOwThe preparation method of the crystal whisker comprises the steps of firstly adding zinc powder into distilled water, adding a proper amount of hydrogen peroxide and mixingStirring for 2-3h by using a motor, standing for 72h at room temperature, filtering, drying for 4-6h at 100 ℃ to obtain pretreated zinc powder, continuously adding the pretreated zinc powder into a melting tank of a melting furnace, melting the zinc powder into a zinc liquid in the melting tank, controlling the temperature in the melting furnace to be 420-wWhisker;
s6, forming of the polymer conductive film: in a three-neck flask equipped with a stirrer and a condenser, the MDP-PPV methanol solution and ZnO are addedwAdding the whisker suspension, glycerol and a parting medium into a flask according to the proportion of 7:3:1:1, heating in water bath at 70-80 ℃ for 25-30min at the rotating speed of 2000-2200r/min, standing at room temperature for 3-5min, filtering, coating on a steel plate, drying in an electrothermal constant-temperature drying oven at 80-90 ℃ for 20-25min, taking out, standing at room temperature for 10min, and removing the membrane to obtain the polymer conductive membrane.
According to the technical scheme, the dispersing agent is prepared from the following raw materials in parts by weight: 35 parts of washing oil, 15 parts of sulfuric acid, 20 parts of formaldehyde, 13 parts of liquid alkali, 5 parts of maleimide, 5 parts of 3-isooctyl mercaptopropionate and 0.4 part of regulating assistant.
According to the technical scheme, the preparation method of the dispersing agent comprises the steps of firstly adding given amount of washing oil into a sulfonation condensation kettle, starting stirring, heating to 60-70 ℃, dropwise adding given amount of sulfuric acid for 1 hour, slowly heating to 115-120 ℃, vacuumizing, keeping the negative pressure at 0.05MPa, keeping the temperature for 2 hours, then cooling to 70 ℃, dropwise adding given amount of formaldehyde, maleimide, 3-isooctyl mercaptopropionate and an adjusting aid for 0.5 hour, sealing equipment after the addition, slowly heating to 80-90 ℃, keeping the temperature for 3-4 hours, keeping the temperature, introducing into a neutralization pot, adding liquid alkali to adjust the pH to 6-7, introducing into a filter press after the adjustment, and drying filtrate in a vacuum drying box at 70-80 ℃ for 2-3 hours to obtain the dispersing agent.
According to the technical scheme, ZnOwThe surface treatment method of the crystal whisker comprises the step of treating ZnOwAdding the crystal whisker into a mixed solution prepared by KH-570 and stearic acid according to the proportion of 2:3, stirring at normal temperature at 800-.
Experimental example:
subject: the polymer conductive film prepared in the embodiment of the invention is used as a first experimental group, a second experimental group and a third experimental group, and a conductive film with common quality on the market, such as a GOLO conductive film, is selected as a first comparison group.
Purpose of the experiment: each set of conductive films was tested for thickness, resistance, breaking strength, and operating temperature.
The experimental method comprises the following steps: according to the national conductive film detection standard and the national standard GB T13541-.
Table of experimental results:
the experimental results show that the polymer conductive film has high breaking strength, good use safety and low resistance, so that the polymer conductive film has better conductivity and can adapt to different environments.
The invention takes MDP-PPV as a film forming matrix and ZnO aswThe crystal whisker is used as a filler, a certain amount of glycerin and a release agent are added at the same time, the MDP-PPV material is a typical conjugated polymer material, and the MDP-PPV material has good film forming property and processability due to high conjugation of a molecular main chain, and ZnO is adoptedwAs a material for preparing a polymer conductive filmThe material has four-needle three-dimensional structure, so that 4 extended needle crystal parts can effectively contact with adjacent needle parts of whiskers to form a good three-dimensional conductive network, so that the material has better conductivity, and ZnOwCompared with metal powder conductive filler, the conductive film has the advantages that the problem of conductivity reduction caused by the formation of an oxide film on the surface of metal particles after long-term use does not exist, the adaptability of the conductive film to the environment is improved, glycerin and a release agent are added during film forming, the formed film is conveniently and quickly removed, and the use convenience is effectively improved.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (3)
1. The processing method of the polymer conductive film is characterized by comprising the following steps: the method comprises the following steps:
s1, Synthesis of 1-methoxy-4 (5' -carboxypentyloxy) benzene: dissolving 400 plus 600ml of sodium hydroxide in ethanol by magnetic stirring and ultrasonic oscillation, slowly dropwise adding the solution into 6-bromohexanoic acid/ethanol solution which is placed in ice water bath and continuously stirred, obtaining white pasty solid after dropwise adding, adding a proper amount of distilled water for dissolving for later use after stirring for 40-45min, firstly introducing ammonia gas for 30min in a three-neck flask which is provided with a stirrer and a reflux condenser tube, adding 100 plus 150ml of sodium hydroxide and distilled water under the protection of the ammonia gas, adding 80-85ml of methoxyphenol and the prepared solution for later use after stirring and dissolving at room temperature, reacting for 22h in an oil bath at 60 ℃, dropwise adding hydrochloric acid for acidification after the reaction is finished, adjusting the pH of the reaction solution to be 1-2, cooling the reaction solution to room temperature, precipitating white solid in the flask, performing suction filtration, repeatedly washing a filter cake to be neutral by the distilled water, vacuum drying at 50 deg.C to obtain white needle sheet crystal, and recrystallizing the obtained solid with anhydrous ethanol to obtain 1-methoxy-4 (5' -carboxypentyloxy) benzene;
synthesis of S2, 1, 4-dibromomethyl-2-methoxy-5 (5' -carboxypentyloxy) benzene: introducing ammonia gas for 0.5h into a three-neck flask provided with a stirrer and a condenser, adding 200-220ml of 1-methoxy-4 (5 '-carboxyl pentoxy) benzene and glacial acetic acid solution, refluxing and stirring for 0.5h under the protection of ammonia gas, after the solution is dissolved, rapidly adding 100-120ml of paraformaldehyde and hydrobromic acid/acetic acid solution, refluxing and reacting for 12h in an oil bath at 85 ℃, pouring the reaction solution into 1000ml of distilled water after the reaction is finished, separating out a large amount of solid, performing suction filtration, repeatedly washing with distilled water until the filter cake is neutral, placing the filter cake at 55 ℃ for vacuum drying to obtain a light yellow granular solid, introducing anhydrous ethanol to dissolve the obtained solid, sequentially washing with a 5% sodium carbonate solution and saturated saline water, and drying with anhydrous sodium sulfate to remove the solvent to obtain the light yellow solid, namely the 1, 4-dibromomethyl-2-methoxy-5 (5' -carboxyl pentoxy) benzene;
s3, synthesis of MDP-PPV: introducing ammonia gas into a three-neck flask provided with a stirrer and a condenser for 0.5h, adding 50-60ml of potassium tert-butoxide and refined anhydrous tetrahydrofuran, stirring and dissolving in an oil bath at 70 ℃, then slowly dropwise adding an anhydrous tetrahydrofuran solution of 1, 4-dibromomethyl-2-methoxy-5 (5' -carboxypentyloxy) benzene, gradually changing the solution into red, slowly deepening the color, after the dropwise adding, continuously heating and stirring for 3-4h, after the reaction is finished, dropwise adding 10ml of distilled water into the reaction liquid, centrifugally separating to obtain a red solid, extracting the red solid with tetrahydrofuran for one week, and vacuum drying at 50 ℃ to obtain a polymer MDP-PPV;
s4, preparing an MDP-PPV methanol solution: putting the polymer MDP-PPV into a vacuum drying oven for drying for 24h, putting the dried polymer MDP-PPV into absolute ethyl alcohol, magnetically stirring for 24h, filtering by a microporous filter to remove insoluble substances, and preparing an MDP-PPV methanol solution;
s5, preparing ZnOwWhisker suspension: 5ml of surface-treated ZnOwAdding whiskers into 30ml of boiling water, and adding 0.25ml of the waterDispersing agent, and maintaining for 45-55min under magnetic stirring to make ZnOwThe crystal whisker is fully dispersed to prepare ZnOwAdding zinc powder into distilled water, adding a proper amount of hydrogen peroxide, stirring for 2-3h by using a motor, standing at room temperature for 72h, filtering, drying at 100 ℃ for 4-6h to obtain pretreated zinc powder, continuously adding the pretreated zinc powder into a melting tank of a melting furnace, melting the zinc powder into a zinc liquid in the melting tank, controlling the temperature in the melting furnace to be 420-750 ℃, introducing the molten zinc liquid into an evaporation tank of a steam generation furnace through a zinc liquid conduit, controlling the temperature in the steam generation furnace to be 1050 ℃ to obtain zinc vapor, introducing the zinc vapor into an oxidation reaction furnace through a zinc vapor conduit after overflowing the evaporation tank, controlling the temperature in the oxidation reaction furnace to be 900-1500 ℃, and contacting the zinc vapor with an oxygen-containing gas in the oxidation reaction furnace to perform oxidation reaction, controlling the reaction gas condition in the oxidation reaction furnace to generate micron or nanometer ZnOw crystal whiskers;
s6, forming of the polymer conductive film: in a three-neck flask equipped with a stirrer and a condenser, the MDP-PPV methanol solution and ZnO are addedwAdding the whisker suspension, glycerol and a parting medium into a flask according to the proportion of 7:3:1:1, heating in water bath at 70-80 ℃ for 25-30min at the rotating speed of 2000-2200r/min, standing at room temperature for 3-5min, filtering, coating on a steel plate, drying in an electrothermal constant-temperature drying oven at 80-90 ℃ for 20-25min, taking out, standing at room temperature for 10min, and removing the membrane to obtain the polymer conductive membrane.
2. The method for processing a polymer conductive film according to claim 1, wherein the dispersant is prepared by adding a predetermined amount of wash oil into a sulfonation condensation kettle, stirring, heating to 60-70 ℃, adding a predetermined amount of sulfuric acid dropwise for 1 hour, slowly heating to 115-120 ℃, vacuumizing, maintaining the negative pressure at 0.05MPa for 2 hours, cooling to 70 ℃, adding a predetermined amount of formaldehyde dropwise for 0.5 hour, sealing the equipment after the addition, slowly heating to 80-90 ℃, maintaining the temperature for 3-4 hours, ending the temperature maintenance, introducing into a neutralization pot, adding alkali to adjust the pH to 6-7, introducing into a filter press after the adjustment, and drying the filtrate in a vacuum drying oven at 70-80 ℃ for 2-3 hours to obtain the dispersant.
3. The method for processing a polymer conductive film according to claim 1, wherein the ZnO iswThe surface treatment method of the crystal whisker comprises the step of treating ZnOwAdding the crystal whisker into a mixed solution prepared by KH-570 and stearic acid according to the proportion of 2:3, stirring at normal temperature at 800-.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4190056A (en) * | 1977-10-31 | 1980-02-26 | General Medical Company | Method and means for recording sweat gland activity |
| CN101962807A (en) * | 2010-10-15 | 2011-02-02 | 北京北矿锌业有限责任公司 | Equipment and method for producing tetrapod-shaped zinc oxide whiskers |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4190056A (en) * | 1977-10-31 | 1980-02-26 | General Medical Company | Method and means for recording sweat gland activity |
| CN101962807A (en) * | 2010-10-15 | 2011-02-02 | 北京北矿锌业有限责任公司 | Equipment and method for producing tetrapod-shaped zinc oxide whiskers |
Non-Patent Citations (1)
| Title |
|---|
| 一种可溶性PPV的合成方法的优化及其应用;李唐卉;《工程科技Ⅰ辑》;20130430 * |
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